JP2682099B2 - Easily soluble baking soda and method for producing the same - Google Patents

Easily soluble baking soda and method for producing the same

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Publication number
JP2682099B2
JP2682099B2 JP1010040A JP1004089A JP2682099B2 JP 2682099 B2 JP2682099 B2 JP 2682099B2 JP 1010040 A JP1010040 A JP 1010040A JP 1004089 A JP1004089 A JP 1004089A JP 2682099 B2 JP2682099 B2 JP 2682099B2
Authority
JP
Japan
Prior art keywords
baking soda
primary particles
particles
less
particle size
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
JP1010040A
Other languages
Japanese (ja)
Other versions
JPH01282118A (en
Inventor
圭一 中矢
邦夫 佐藤
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
AGC Inc
Original Assignee
Asahi Glass Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Asahi Glass Co Ltd filed Critical Asahi Glass Co Ltd
Publication of JPH01282118A publication Critical patent/JPH01282118A/en
Application granted granted Critical
Publication of JP2682099B2 publication Critical patent/JP2682099B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D7/00Carbonates of sodium, potassium or alkali metals in general
    • C01D7/38Preparation in the form of granules, pieces or other shaped products
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D7/00Carbonates of sodium, potassium or alkali metals in general
    • C01D7/35Varying the content of water of crystallisation or the specific gravity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Glanulating (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Detergent Compositions (AREA)

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は易溶性重曹及びその製造方法、特に血液透析
液等の医薬品あるいは食品などの用途に適する易溶性で
取り扱いの容易な重曹に係るものである。
DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to an easily soluble baking soda and a method for producing the same, and particularly to an easily soluble and easy-to-handle baking soda suitable for use in pharmaceutical products such as hemodialysis fluid or foods. Is.

(従来の技術) 重曹は一般に粉体として取り扱われており、用途によ
って各種の粉体特性、例えば流動性,粒子の大きさ,嵩
比重,溶解性等を有するものが要求される。
(Prior Art) Baking soda is generally handled as a powder, and it is required to have various powder characteristics such as fluidity, particle size, bulk specific gravity, and solubility depending on the application.

これら重曹の製法としては、炭酸ソーダを含む水溶液
を重炭酸化するか、あるいは重曹を含む溶液を冷却する
かして重曹結晶を析出せしめる方法が一般的である。
As a method for producing these baking sodas, a method of precipitating sodium bicarbonate crystals by bicarbonate of an aqueous solution containing sodium carbonate or by cooling a solution containing sodium bicarbonate is common.

(発明が解決しようとする課題) しかしながら、これらの方法によって得られる重曹
は、針状あるいは板状になり易く、微小粒子であるた
め、流動性に乏しく、嵩比重が小さく、取り扱い難いも
のであるのが一般的であった。
(Problems to be Solved by the Invention) However, the baking soda obtained by these methods is likely to be needle-shaped or plate-shaped, and since it is fine particles, it has poor fluidity, has a low bulk specific gravity, and is difficult to handle. Was common.

これらの物性のうち流動性は各用途共に取扱い上重要
な要素である。この為、流動性を改善せんものとして例
えば媒晶剤を用いたり、析出条件等を特定化して結晶の
形状や大きさを制御することが提案されている。(例え
ば特公昭48−17160号,特開昭55−60021号,特開昭60−
60925号各公報参照)しかしながら、これらの方法は確
かに流動性の改善には有効ではあるが、溶解や反応を行
なわしめる用途に対しては逆に溶解速度や反応速度が著
しく低下する欠点を有している。
Among these physical properties, fluidity is an important factor in handling in each application. Therefore, it has been proposed to use a habit modifier, for example, as a material for improving the fluidity, or to control the shape and size of the crystal by specifying the precipitation conditions and the like. (For example, JP-B-48-17160, JP-A-55-60021, JP-A-60-
However, although these methods are certainly effective in improving the fluidity, they have the drawback that the dissolution rate and reaction rate are markedly reduced for applications in which dissolution or reaction is performed. doing.

また、有機質のバインダーを用いて重曹を造粒するこ
とにより流動性と溶解性の両方の特性を改善することも
考えられているが、この場合造粒物に有機質のバインダ
ーが残ってしまうという問題点がある。
It is also considered to improve both the fluidity and the solubility by granulating baking soda with an organic binder, but in this case the problem that the organic binder remains in the granulated product There is a point.

(課題を解決するための手段) 本発明者は、これら従来法が有している欠点を排除
し、十分な流動性と共に易溶性をも兼ね備えた重曹を得
ることを目的として種々研究,検討した結果、重曹を特
定の物性を有する顆粒状にすることにより前記目的を達
成し得ることを見出した。かくして本発明は、有機質の
バインダーを含まず実質的に重曹の組成から成り、結晶
性1次粒子が凝集結合した顆粒状重曹であって、その溶
解時間が1次粒子の溶解時間の3倍以下であり、摩耗率
が50%以下であり、安息角が50度以下である易溶性重曹
およびその製造方法を提供するものである。
(Means for Solving the Problem) The present inventor has conducted various studies and studies for the purpose of eliminating the drawbacks of these conventional methods and obtaining baking soda having both sufficient fluidity and easy solubility. As a result, they have found that the above objects can be achieved by making baking soda into granules having specific physical properties. Thus, the present invention is a granular baking soda which does not contain an organic binder and is substantially composed of baking soda, and in which crystalline primary particles are cohesively bonded, and the dissolution time thereof is not more than 3 times the dissolution time of the primary particles. And a wear rate of 50% or less and a repose angle of 50 degrees or less, and a method for producing the same.

本発明において、溶解時間とは次の様に定義される。
容量1のビーカーに500mlの水を入れ、25℃に保持
し、54mmφのプロペラ型撹拌浴を持つ撹拌機にて600r.
p.mで撹拌しつつ、試料50gをビーカーに投入し、その90
%が溶解した時間をもって溶解時間とする。溶解量は溶
液を撹拌しながら、定期的にその一部を少量ずつサンプ
リングして分析することにより求める。
In the present invention, the dissolution time is defined as follows.
Put 500 ml of water in a beaker with a capacity of 1 and keep it at 25 ° C.
While stirring at pm, add 50 g of sample to a beaker,
The time when the% is dissolved is defined as the dissolution time. The dissolved amount is obtained by periodically sampling a portion of the solution while agitating the solution and analyzing it.

また、摩耗率とは次の様に定義される。試料30gを100
または65または32メッシュのいずれか1つの標準篩(直
径20cm)に入れ、軽く篩ってその目開き以下の粒径の2
次粒子を取り除き残った粒子の重量を測定し、これをA
とする。次に篩上に粒子を入れたまま篩の面を水平に保
ち、篩の面に並行に直径15mmの円を描くように200回転
/分で1時間振動させる。この振動のため篩上で破砕し
て篩を通過した粒子の重量を測定し、これをBとする。
B/Aの割合を%で表示し、これを摩耗率とする。ここで
篩は、以下のように粒径に応じて選ぶ。あらかじめ2次
粒子の粒径分布を測定して粒径の小さい方から10重量%
に相当する粒径を求めておく。その粒径が210μ未満の
場合は100メッシュの篩を用いる。その粒径が210μ以上
500μ未満の場合は65メッシュの篩を用いる。その粒径
が500μ以上の場合は32メッシュの篩を用いる。
The wear rate is defined as follows. 30 g of sample to 100
Or, put it in one of the standard sieves (diameter 20 cm) of 65 or 32 mesh, sieve it lightly, and
The next particles were removed and the weight of the remaining particles was measured.
And Next, the surface of the sieve is kept horizontal while the particles are put on the sieve, and the surface of the sieve is vibrated at 200 rpm for 1 hour so as to draw a circle having a diameter of 15 mm in parallel. Due to this vibration, the particles that were crushed on the sieve and passed through the sieve were weighed and designated as B.
The ratio of B / A is displayed in%, and this is taken as the wear rate. Here, the sieve is selected according to the particle size as follows. Measure the particle size distribution of the secondary particles in advance and from the smaller particle size, 10% by weight
The particle size corresponding to is calculated. If the particle size is less than 210μ, use a 100 mesh screen. The particle size is 210μ or more
If it is less than 500μ, use a 65 mesh screen. If the particle size is 500μ or more, use a 32 mesh screen.

また、安息角は底面限定法による。本明細書において
は、細川ミクロン(株)製のパウダーテスターで測定し
た値である。
The angle of repose is based on the bottom-only method. In the present specification, it is a value measured by a powder tester manufactured by Hosokawa Micron Co., Ltd.

かくして本発明による重曹は、有機質のバインダーを
含まず実質的に重曹の組成から成り、結晶性1次粒子
(以下1次粒子という)が凝集結合した顆粒状重曹(以
下2次粒子という)の形態となっている。本発明の顆粒
状重曹は、重曹が97重量%以上、好ましくは99重量%以
上含まれていることが好適である。本発明において1次
粒子に存在していても特に差し支えない重曹以外の成分
は、炭酸ソーダあるいはセスキ炭酸ソーダである。
Thus, the baking soda according to the present invention has a composition of substantially baking soda without containing an organic binder, and is in the form of granular baking soda (hereinafter referred to as secondary particles) in which crystalline primary particles (hereinafter referred to as primary particles) are cohesively bonded. Has become. The granular baking soda of the present invention preferably contains 97% by weight or more, and preferably 99% by weight or more of baking soda. In the present invention, the components other than baking soda which may be present in the primary particles are sodium carbonate or sodium sesquicarbonate.

かかる重曹を構成する結晶性1次粒子は、粒子径100
μ以下の粒子が60重量%以上、望ましくは90重量%以上
であることが好ましい。1次粒子の粒子径が100μを超
えたものが多く存在する程、摩耗率が高くなり、また溶
解時間が長くなる。
The crystalline primary particles constituting such baking soda have a particle size of 100.
It is preferable that the particles of μ or less are 60% by weight or more, and desirably 90% by weight or more. The greater the number of primary particles having a particle size of more than 100 μ, the higher the wear rate and the longer the dissolution time.

また、1次粒子の平均アスペクト比について、4以
下、より好適には2以下を採用する場合は、摩耗率の低
下を防ぐことが出来るので好ましい。
Further, when the average aspect ratio of the primary particles is 4 or less, more preferably 2 or less, it is possible to prevent the wear rate from decreasing, which is preferable.

本発明による易溶性顆粒状重曹は、その物性として溶
解時間が1次粒子のそれの3倍以下である必要がある。
溶解時間が3倍を超える場合には、1次粒子に比べて溶
解性が低下しすぎるので不適当である。
The easily soluble granular baking soda according to the present invention has a physical property that the dissolution time is not more than 3 times that of the primary particles.
When the dissolution time exceeds 3 times, the solubility is too low as compared with the primary particles, which is not suitable.

また、摩耗率が50%以下である必要がある。これが50
%を超える場合には、輸送等の取り扱い過程で2次粒子
が崩壊し、1次粒子そのものとなり、飛散したりして使
用時に取り扱いが困難となるので不適当である。
Also, the wear rate must be 50% or less. This is 50
If it exceeds%, the secondary particles are disintegrated during the handling process such as transportation to become the primary particles themselves, and the particles are scattered, making it difficult to handle at the time of use.

また、安息角は50度以下である必要がある。安息角が
前記範囲を超える場合には、流動性が悪くなり、例えば
他の固体材料と均一に混合することが困難となるので不
適当である。
Also, the angle of repose should be 50 degrees or less. When the angle of repose exceeds the above range, the fluidity is deteriorated, and it becomes difficult to uniformly mix with other solid materials, which is not suitable.

2次粒子の平均粒子径としては、0.1〜5mmが好まし
い。平均粒子径が前記範囲に満たない場合には流動性が
悪く、逆に前記範囲を超える場合には摩耗強度が低下す
る虞れがあるので何れも好ましくない。
The average particle diameter of the secondary particles is preferably 0.1 to 5 mm. If the average particle size is less than the above range, the fluidity is poor, and conversely, if it exceeds the above range, the abrasion strength may decrease, which is not preferable.

本発明の易溶性顆粒状重曹を製造する方法としては、
例えば次の様な方法が好ましい。
As a method for producing the easily soluble granular baking soda of the present invention,
For example, the following method is preferable.

先ず、結晶性1次粒子からなる原料重曹粉末に、水分
が0.5〜10重量%となる様に液体を混合して造粒する。
加える水分の量が前記範囲に満たない場合には2次粒子
の摩耗率が大きくなり、逆に前記範囲を超える場合には
造粒が困難となるので何れも好ましくない。
First, a raw material baking soda powder consisting of crystalline primary particles is mixed with a liquid so as to have a water content of 0.5 to 10% by weight, and granulated.
If the amount of water added is less than the above range, the wear rate of the secondary particles becomes large, and conversely, if it exceeds the above range, granulation becomes difficult, which is not preferable.

造粒時に加える液体としては、水を用いることもでき
るが、造粒物の1次粒子間に存在する液相として炭酸ソ
ーダ水溶液が形成されるような液体を用いる場合は、後
述の乾燥工程において重曹1次粒子間においてこの水溶
液中の炭酸ソーダと炭酸ガスとが反応して新たな重曹が
析出し、1次粒子間の結合強度が向上するため摩耗率を
低減できるので好ましい。
Water can be used as the liquid added at the time of granulation, but when a liquid that forms an aqueous solution of sodium carbonate is formed as the liquid phase existing between the primary particles of the granulated product, it is used in the drying step described below. The sodium carbonate in the aqueous solution reacts with carbon dioxide gas between primary particles of baking soda to deposit new baking soda, and the bond strength between the primary particles is improved, so that the wear rate can be reduced, which is preferable.

この水溶液の濃度は、フェノールフタレンで着色する
程度でも有効であるが、炭酸根が1〜19重量%の濃度に
なるようにするのが効果的である。この液体としては炭
酸ソーダ水溶液が好ましい。また、苛性ソーダ水溶液を
用いても造粒の際に苛性ソーダと重曹1次粒子が反応し
て1次粒子の間には炭酸ソーダ水溶液ができるので、始
めから炭酸ソーダ水溶液を用いるのと同じ効果を得るこ
とができる。同様に、セスキ炭酸ソーダなどの水溶液を
用いることもできる。
The concentration of this aqueous solution is effective even if it is colored with phenolphthalene, but it is effective to adjust the concentration of carbonate to 1 to 19% by weight. An aqueous solution of sodium carbonate is preferable as this liquid. Even when an aqueous solution of caustic soda is used, sodium hydroxide reacts with primary particles of sodium bicarbonate during granulation to form an aqueous solution of sodium carbonate between the primary particles, so that the same effect as using the aqueous solution of sodium carbonate can be obtained from the beginning. be able to. Similarly, an aqueous solution of sodium sesquicarbonate or the like can be used.

かかる条件に基づき実施される具体的造粒手段として
は、例えば湿式転動造粒、押出し造粒が適当であり、圧
縮成形法による造粒のように1次粒子が破壊されたり圧
縮固化されるような手段は、溶解時間が長くなるため好
ましくない。
As specific granulation means carried out under such conditions, for example, wet rolling granulation and extrusion granulation are suitable, and primary particles are broken or compressed and solidified as in granulation by a compression molding method. Such means is not preferable because the dissolution time becomes long.

造粒された粒子は次いで炭酸ガス雰囲気中で乾燥さ
れ、本発明の易溶性顆粒状重曹が得られる。この場合、
炭酸ガス雰囲気中の炭酸ガス濃度としては、乾燥時の重
曹の分解防止及び炭酸ソーダ分の重炭酸化を十分たらし
める理由から5%以上を採用するのが適用である。ま
た、この場合の乾燥温度としては30〜90℃程度を採用す
るのが適当である。
The granulated particles are then dried in a carbon dioxide gas atmosphere to obtain the easily soluble granular baking soda of the present invention. in this case,
As the carbon dioxide concentration in the carbon dioxide atmosphere, it is appropriate to adopt 5% or more for the purpose of preventing decomposition of sodium bicarbonate during drying and sufficiently causing bicarbonate of the sodium carbonate content. In this case, it is appropriate to adopt a drying temperature of about 30 to 90 ° C.

かかる条件に基づき実施される具体的乾燥手段として
は、例えばバンド乾燥機、回分式箱型乾燥機、円板乾燥
機、通気乾燥機、回転乾燥機等が挙げられる。
Specific drying means carried out under such conditions include, for example, a band dryer, a batch-type box dryer, a disk dryer, an aeration dryer, a rotary dryer and the like.

(実施例) 公知の方法によって得られた平均粒径50μであって、
粒子径100μ以下の粒子が90%存在し、平均アスペクト
比が2の重曹結晶1次粒子10kgに、炭酸根を12重量%含
有する炭酸ソーダ水溶液0.71Kgを添加し、重曹の水分が
5重量%となるように混合した。次に、これを双軸型押
し出し造粒機を用いて造粒し、平均粒径400μの造粒物
を得た。次いで炭酸ガス濃度20%、温度50℃に調整され
た熱風循環型乾燥機に前記造粒物を入れ、3時間乾燥せ
しめた。
(Example) An average particle size of 50μ obtained by a known method,
90% of particles having a particle size of 100μ or less are present, and 0.71 Kg of sodium carbonate aqueous solution containing 12% by weight of carbonate root is added to 10 kg of primary particles of sodium bicarbonate crystals having an average aspect ratio of 2, and the water content of baking soda is 5% by weight. Mixed so that Next, this was granulated using a twin-screw type extrusion granulator to obtain a granulated product having an average particle size of 400μ. Next, the granulated product was placed in a hot air circulation type dryer adjusted to a carbon dioxide gas concentration of 20% and a temperature of 50 ° C. and dried for 3 hours.

この結果、顆粒状の2次粒子からなる重曹が得られ
た。その平均粒子径は、0.4mmであり、溶解時間は原料
重曹(1次粒子)の1.3倍であり、65メッシュの標準篩
を用いて測定した摩耗率3%、細川ミクロン(株)製の
パウダーテスターで測定した安息角は38度であった。そ
してかかる2次粒子は通常の取り扱いでは粉化せず、ま
た溶解に際して取扱いも容易であり、しかも極めて容易
に25℃の水に溶解した。
As a result, baking soda composed of granular secondary particles was obtained. Its average particle size was 0.4 mm, dissolution time was 1.3 times that of raw baking soda (primary particles), wear rate was 3% measured using a standard 65 mesh sieve, powder from Hosokawa Micron Co., Ltd. The angle of repose measured by a tester was 38 degrees. The secondary particles were not pulverized by normal handling, were easy to handle when dissolved, and were extremely easily dissolved in water at 25 ° C.

Claims (7)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】有機質のバインダーを含まず実質的に重曹
組成から成り、結晶性1次粒子(以降1次粒子と称す)
が凝集結合した顆粒状重層(以降2次粒子と称す)であ
って、2次粒子の溶解時間が1次粒子の溶解時間の3倍
以下であり、摩耗率が50%以下であり、安息角が50度以
下である易溶性重曹。
1. Crystalline primary particles (hereinafter referred to as primary particles) which are substantially composed of sodium bicarbonate and do not contain an organic binder.
Are cohesively bonded granular multilayers (hereinafter referred to as secondary particles), the dissolution time of the secondary particles is 3 times or less than the dissolution time of the primary particles, the wear rate is 50% or less, and the angle of repose is Soluble baking soda with a melting point of 50 degrees or less.
【請求項2】1次粒子は、粒子径100μ以下の粒子が60
重量%以上である請求項1の重曹。
2. Primary particles are 60 particles having a particle size of 100 μm or less.
The baking soda according to claim 1, wherein the baking soda is at least wt%.
【請求項3】1次粒子の平均アスペクト比が4以下であ
る請求項1または2の重曹。
3. The baking soda according to claim 1 or 2, wherein the average aspect ratio of the primary particles is 4 or less.
【請求項4】2次粒子の平均粒子径が0.1〜5mmである請
求項1〜3いずれか1の重曹。
4. The baking soda according to claim 1, wherein the secondary particles have an average particle size of 0.1 to 5 mm.
【請求項5】実質的に重曹から成る結晶性1次粒子を、
水分が0.5〜10重量%となる様に液体と混合造粒し、炭
酸ガス雰囲気中で乾燥することを特徴とする易溶性重曹
の製造方法。
5. A crystalline primary particle consisting essentially of baking soda,
A method for producing a readily soluble baking soda, which comprises mixing and granulating with a liquid so that the water content is 0.5 to 10% by weight, and drying in a carbon dioxide gas atmosphere.
【請求項6】混合する液体が、重曹と混合したとき造粒
物の1次粒子間に存在する液相として炭酸ソーダ水溶液
が形成されるような液体である請求項5の製造方法。
6. The method according to claim 5, wherein the liquid to be mixed is a liquid which forms an aqueous solution of sodium carbonate as a liquid phase existing between the primary particles of the granulated product when mixed with sodium bicarbonate.
【請求項7】造粒の方法が、押し出し造粒である請求項
5または6の重曹の製造方法。
7. The method for producing baking soda according to claim 5, wherein the granulation method is extrusion granulation.
JP1010040A 1988-01-22 1989-01-20 Easily soluble baking soda and method for producing the same Expired - Fee Related JP2682099B2 (en)

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JP63-10913 1988-01-22

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JP2682099B2 true JP2682099B2 (en) 1997-11-26

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Publication number Priority date Publication date Assignee Title
ATE340762T1 (en) * 2002-03-29 2006-10-15 Asahi Glass Co Ltd METHOD FOR PRODUCING CRYSTALLINE PARTICLES FROM SODIUM HYDROGEN CARBONATE WITH LOW ADHESIVE PROPERTIES, AND SUCH PARTICLES

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